反应详情

To a solution of 3271 g of sodium hydroxide in 33,000 ml of water is added 3271 g of 1-(4-acetamidocyclohexyl)-2-imidazolidinone. The mixture is stirred and refluxed for 4 hours. The reaction mixture is cooled to room temperature and 3271 g of sodium chloride is added with stirring. The reaction mixture is extracted a total of 10 times using a total volume of 93,000 ml of dichloromethane. The dichloromethane solution containing the product is concentrated in vacuo to a volume of about 5 liters. To this solution is added 300 g of magnesium sulfate, anhydrous. The mixture is stirred at room temperature for about 3 hours, filtered and the filtrate concentrated in vacuo to dryness. The resulting residue is dried in high vacuum to constant weight to give 1-(4-aminocyclohexyl)-2-imidazolidinone, as a mixture of isomers which crystallizes on standing at room temperature.

1. temperaturerefluxed for 4 hours
2. stirringwith stirring
3. extractionThe reaction mixture is extracted a total of 10 times
4. additionThe dichloromethane solution containing the product
5. concentrationis concentrated in vacuo to a volume of about 5 liters
6. additionTo this solution is added 300 g of magnesium sulfate
7. stirringThe mixture is stirred at room temperature for about 3 hours
8. filtrationfiltered
9. concentrationthe filtrate concentrated in vacuo to dryness
10. customThe resulting residue is dried in high vacuum to constant weight